KR101877874B1 - Manufacturing method of methyl 3-methoxypropionate with high purity and yield and manufacturing equipment therefor - Google Patents

Abstract

The present invention relates to a process for producing methyl 3-methoxypropionate of high purity and high yield and an apparatus for producing the same which optimize the process. In the reaction process of methanol and methyl acrylate, And to provide a process and apparatus for producing a high-yield product.

Description

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a process for preparing methyl 3-methoxypropionate having high purity and high yield,

The present invention relates to a process for producing methyl 3-methoxypropionate of high purity and high yield and an apparatus for producing the same which optimize the process. In the reaction process of methanol and methyl acrylate, And to provide a process and apparatus for producing a high-yield product.

Alkylalkoxypropionate is known as a variety of industrial solvents such as coatings, paints, and inks, and is also used in various processes as a solvent capable of dissolving various solutes in semiconductor processing.

The preparation of alkylalkoxypropionates has been studied for quite some time and many methods are known.

In the presence of an acid catalyst such as sulfuric acid, zinc chloride, aluminum chloride or boron trifluoride, by reacting the corresponding dialkoxymethane with ketene. However, this method has many undesired side reactants such as alkyl acetate, alkoxymethyl acetate, and the impurity providing process is difficult. Further, in order to increase the yield, ketene and dialkoxy must be reacted at a relatively low temperature of 0 ° C or lower, which causes a problem in that the process becomes complicated. Thus, studies have been made on how to carry out the process at higher temperatures, one of which has been presented in the form of anhydrous condition and a specific form of boron triple fluoride as catalyst. In the case of using zinc chloride as a catalyst, there are also patents which suggest another condition. However, boron triple fluoride is expensive in comparison to other proton acids and is causing problems with corrosion, toxicity and waste treatment. As a specific form of alkylalkoxypropionate, a method of using hexafluorophosphoric acid as a catalyst in a more optimized form of production of methyl 3-methoxypropionate has been proposed, but the reaction temperature is still low, This is complicated.

Although not applicable to the preparation of methyl 3-methoxypropionate, it has been found that, in the process for preparing alkylalkoxypropionates having at least 7 carbon atoms, the basic reaction for the reaction of dialkoxymethane with ketene is maintained and alkylcarboxylic anhydride and fumarate A method of using sulfuric acid as a catalyst is also disclosed. Fuming sulfuric acid absorbs a large amount of sulfur trioxide in 98% of concentrated sulfuric acid. It is named after it is always producing sulfur trioxide vapor and producing white smoke in air.

On the other hand, a relatively simple but relatively high yielding method has been proposed for the production of methyl 3-methoxypropionate. Methanol and methyl acrylate are reacted with an alkali metal alkoxide as a catalyst. The reaction is carried out by adding an alcohol to the double bond of the acrylate ester in the presence of a strong base catalyst. In this regard, the foreign documents as well as the domestic patent publication No. 10-2001-0019332 disclose contents related thereto. According to Korean Patent Laid-Open No. 10-2001-0019332, reaction is carried out using methanol and methyl acrylate as starting materials, and an alkali metal alkoxide, especially sodium methoxide, is used as a catalyst, and the reaction temperature is in the range of 40 to 70 ° C . Further, it is mentioned that after the reaction, sulfuric acid is poured into the reactant to neutralize the alkali metal alkoxide used as a catalyst, so that a high yield can be obtained by preventing the reverse reaction after distilling off excess methanol.

However, although it is said that this method is a relatively simple method of high yield, it is not easy to obtain a high yield in practice. First, the material used as a catalyst may not be active in the presence of moisture because it is very sensitive to moisture. Methanol and methyl acrylate have to be of high quality anhydrous form and have to go through a very expensive process and are not actually produced using this method.

However, there have been researches and developments on a mode in which the process of this method is modified and used again. In other words, a strong acid such as benzenesulfonic acid or toluenesulfonic acid is used as a catalyst, but the reaction temperature is raised to 120 to 130 ° C, which is relatively high, without using an alkaline metal alkoxide sensitive to moisture as a catalyst. Since the boiling point of the alcohol is much lower than the above-mentioned temperature, there is a part where the pressurization condition is required in the reaction. The problem with this process, however, is the subsequent reaction of the dialkyl ether in the condensation of the alcohol. Another problem is that a polymerization reaction of alkyl acrylate can occur, and therefore a polymerization inhibitor should be used.

US 2,910,503 US 3,134,807 US 4,785,133 KR 10-2001-0019332A

Disclosure of Invention Technical Problem [8] Accordingly, the present invention has been made to solve the above-mentioned problems, and it is an object of the present invention to provide a process capable of suppressing side reactions through a process such as moisture control during a reaction sampling process between methanol and methyl acrylate, ≪ / RTI >

To this end, the present invention provides a method for producing methyl methoxypropionate (MMP) by reacting methyl acrylate with methanol using an alkali metal alkoxide as a catalyst, wherein water is added to the reaction so as to increase the conversion of the MMP And further comprising a step of supplying and reacting the MMP.

Then, the reaction is first sampled between 20 minutes and 45 minutes after the start of the reaction, and the conversion rate and moisture of the MMP are measured to determine whether water is additionally supplied or not.

The supply of the moisture is preferably in the range of 100 ppm to 200 ppm.

If the MMP conversion rate is 98% or less, the conversion of the MMP can be increased by repeating the process of further feeding moisture to the reaction and conducting the reaction.

The alkali metal alkoxide catalyst is preferably sodium methoxide.

The present invention also relates to a process for the preparation of a compound of formula (I), comprising the steps of: i) reacting methyl acrylate with methanol using sodium methoxide as a catalyst; Ii) sampling the reaction of step i) to determine whether additional moisture is supplied; Iii) supplying additional water and reacting according to the determination of step ii); Iv) neutralizing the catalyst by addition of acid; And (v) distilling the reaction product. The present invention also provides a process for producing methylmethoxypropionate (MMP).

The present invention relates to an apparatus for producing methyl methoxypropionate (MMP) by reacting methyl acrylate with methanol using an alkali metal alkoxide as a catalyst, the apparatus comprising a synthesis control unit, a neutralization control unit, A synthesis reactor, a MAM feeder for feeding methyl acrylate monomer, a methanol feeder for feeding methanol, a catalyst feeder for feeding the catalyst, a reactor for feeding the catalyst, And a moisture supplier for supplying water to the synthesis reactor.

The neutralization control unit includes a neutralization reactor and a neutralizer feeder, and the synthesized material is sent to the neutralization controller to neutralize the catalyst.

The first distillation unit includes a first evaporator, a first distillation column, a first condenser, a second condenser, and a first cooler. The first condenser receives the neutralization reactant from the neutralization controller, And distillation is carried out.

The second distillation unit includes a second evaporator, a second distillation column, a third condenser, a fourth condenser, a second condenser, and a third condenser, and the second distillation unit is not distilled from the first distillation unit And the second distillation is carried out.

The production method and apparatus of the present invention can provide methyl 3-methoxypropionate of high purity and high yield and can easily accomplish this without any fine control of the process, and it has little side reaction and easily removes impurities It is a process and equipment that can be done.

BRIEF DESCRIPTION OF THE DRAWINGS FIG. 1 is a schematic view showing a reaction process of a synthesis control unit as a part of an apparatus for producing methyl methoxypropionate according to the present invention. FIG.
FIG. 2 is a schematic view showing a reaction process of the neutralization control unit as part of an apparatus for producing methyl methoxypropionate according to the present invention. FIG.
3 is a schematic diagram showing a first distillation apparatus section as a part of an apparatus for producing methyl methoxypropionate according to the present invention.
FIG. 4 is a schematic view showing a second distillation unit as a part of an apparatus for producing methyl methoxypropionate according to the present invention. FIG.

In the process for producing methyl 3-methoxypropionate (MMP) of the present invention, methanol is reacted with methylacrylate monomer (MAM) as shown in the following reaction formula 1, and an alkali such as sodium methoxide Metal alkoxide is used as a reaction catalyst.

<Reaction Scheme 1>

The reaction is a well known reaction, with a typical yield of 54%. The conversion of MAM can be increased by controlling the reaction temperature, controlling the catalyst, neutralizing reaction, etc., and the purity can be increased by recycling the distillation procedure. The reaction is an exothermic reaction in which a cooler is installed in the reactor to control the temperature. Sodium methoxide is dissolved in methanol and used. Methanol and sodium methoxide dissolved in methanol are added to the reactor, and MAM is slowly added dropwise to react. The temperature of the droplet is suitably about 40 DEG C, and the reaction is an exothermic reaction in which a cooler is installed in the reactor to adjust the temperature.

The drop-in time is about 10 minutes. As an exothermic reaction, when the temperature change of the reactor was observed, the temperature increased until about 20 minutes after the start of the reaction. If so, it can be assumed that the reaction is actually in equilibrium from the 20th minute, and even if the reaction time is increased, there is no change in the equilibrium state if there is no change in other conditions. Therefore, some changes are needed so that the reaction proceeds to the right.

The conversion of methylacrylate to methanol in the same molar amount and in the case of an excessive amount of methanol shows a considerable difference, so that an excessive amount of methanol is an important factor that significantly increases the conversion rate. However, even when methanol is excessively charged and various conditions are optimized, there is a limit to maximization of the conversion rate. It is difficult to grasp the appropriate level of factors to be adjusted for each stage of each process and it is not easy to cope with each of them. When the recycle of the reaction procedure is carried out, it is difficult to grasp the condition at the time of recycling and it is not easy to maximize the efficiency. It is necessary to simplify the control of the process conditions and to simplify factors that affect the process.

In the present invention, it has been found that adding water after a certain degree of reaction changes the equilibrium of the reaction. In general, the reaction of Scheme 1 may be less active in the presence of water because the catalyst is very sensitive to moisture. Thus, methanol and methyl acrylate are preferably in a relatively high-quality anhydrous form. Therefore, in the present invention, it seems unreasonable that the addition of water increases the reactivity. The reaction is carried out by adding an alcohol to the double bond of the acrylate ester in the presence of a strong base catalyst. The higher the nucleophilicity, the more likely the reaction will be. The addition of H ₂ O can raise the nucleophilicity of the nucleophile. On the other hand, it is contradicted that the presence of moisture inhibits the activity of the strong base catalyst, which is undesirable. In the present invention, a method of adding water after chemical equilibrium has been achieved after the reaction has progressed to a certain degree has been selected. Even if the chemical equilibrium state is established, the addition of water will undesirably decrease the activity of the catalyst. Rather, it increases the hydrogen ions and methoxide ions and increases their activity, thereby shifting the reaction to the right. Sodium methoxide has a high reactivity with moisture, thus producing an ionized state of H ₂ O. Due to the strong binding force between the sodium ion and the hydroxide ion rather than the binding force between the hydrogen ion and the methoxide ion, the hydrogen ion and the methoxide are converted into particles having energy greater than the activation energy, .

While the reaction under sodium methoxide catalyst will vary depending on other conditions, the chemical equilibrium appears to be approximately 20 to 25 minutes after the reaction. That is, even if the reaction is continued for 2 or 3 hours, the conversion rate is the same. Therefore, the chemical equilibrium is in a state of a certain degree at about any point between 20 minutes and 45 minutes after the start of the reaction. Therefore, in order to increase the conversion rate, it is necessary to supply water at this time to further proceed the positive reaction. It is a technical point of the present invention that the chemical equilibrium can be progressed in a proper manner by injecting water at a time point where the chemical equilibrium is made to some extent and there is no change. The reaction time after the addition of water is suitably about 20 minutes, and it is a time that the reaction by water addition can sufficiently take place. On the other hand, among alkali metal alkoxides having a strong basicity as a catalyst, sodium metal alkoxide is more preferably used as the alkali metal alkoxide because it is expected to further show the above-mentioned specificity when alkali metal methoxide is used.

In the present invention, 98% or more is preferably aimed at the conversion rate. The reaction temperature and an excess amount of methanol can achieve a conversion of some degree or more, but a conversion of about 90% or so can be achieved. Optimization of several conditions may achieve up to 95%, but it is not easy to adjust these conditions and it is not easy to optimize all of the various factors. Accordingly, the present invention has an advantage that it is possible to increase the conversion rate through addition of only a few percent of methanol without strictly adjusting the reaction temperature and the appropriate excess amount of methanol, thereby greatly facilitating the process control. That is, the reactant is sampled and the conversion rate to MMP is measured. When the amount of the reaction is less than 98%, water is added. It is preferable that the water content is in the range of 100 ppm to 200 ppm. If the content of water is too small, it is difficult to achieve the expected effect, and the content of water more than necessary may deteriorate the reactivity. In the sampling process in which a part is collected in the reactor, the conversion rate is measured by GC, the water content (Karl-fisher method) is confirmed by a moisture meter, and the reaction is performed according to the moisture content in the above range. After the water is added and reacted, the sample is re-sampled, and if the conversion to MMP is 98% or less, the above procedure can be repeated to increase the conversion rate. When the reaction is completed, the reactor is cooled to about 30 to 40 DEG C by lowering the temperature of the reactor.

In the present invention, the molar ratio of adding methanol and MAM is preferably about 2 moles of methanol per 1 mole of MAM. An excess of methanol promotes the reaction, and approximately 1.5 to 2.5 moles is safe. In the case of the catalyst, the amount is preferably about 0.005 mole based on 1 mole of MAM, and preferably about 0.002 mole to about 0.01 mole. In the state of chemical equilibrium, excess methanol is present, and therefore, it is distilled to remove it. If the methanol is reduced during the distillation process, the chemical equilibrium will be shifted to the left, and the yield of the MMP may be lowered. Therefore, by neutralizing the reaction catalyst before the distillation process, the activation energy barrier is increased to prevent the reverse reaction shall. It can be neutralized using 50% H ₂ SO ₄ in MeOH. The neutralization is allowed to react for about 30 minutes.

When the neutralization is complete, the reaction product is distilled. MMP, MAM, sulfuric acid, and the like are present together with the reactant including methanol added in an excess amount. The boiling point of methanol is about 64.7 ° C, the boiling point of MAM is 80.5 ° C, the boiling point of MMP is about 143 ° C, and the boiling point of sulfuric acid is about 317 ° C. Since methanol and MMP should be separated from each other, it is necessary to carry out a second distillation process.

The present invention relates to a process for the preparation of a compound of formula (I), which comprises: i) reacting methyl acrylate with methanol using sodium methoxide as a catalyst; Ii) sampling the reaction of step i) to determine whether additional moisture is supplied; Iii) supplying additional water and reacting according to the determination of step ii); Iv) neutralizing the catalyst by addition of acid; And (v) distilling the reaction product. The present invention also provides a process for producing methylmethoxypropionate (MMP).

The present invention also discloses a preferred form of apparatus for producing methyl methoxypropionate (MMP) by reacting methyl acrylate with methanol using an alkali metal alkoxide as a catalyst. 1 to 4 are schematic views of a synthesis control device, a neutralization control device, a first distillation device, and a second mainstream device, respectively. In order to clarify the gist of the present invention, Vacuum apparatuses, hot water or cold water inlet for heating or cooling, display of outlets, and various control apparatuses are omitted.

BRIEF DESCRIPTION OF THE DRAWINGS FIG. 1 is a schematic view showing a reaction process of a synthesis control unit as a part of an apparatus for producing methyl methoxypropionate according to the present invention. FIG. The reaction takes place in the synthesis reactor (100). Methanol may be supplied via the methanol feeder 120 and sodium methoxide may be fed to the synthesis reactor 100 via the catalyst feeder 130. The methanol feeder 120 and the catalyst feeder 130 are interlocked to supply the synthesis methane to the synthesis reactor 100 in a state where sodium methoxide is dissolved in methanol. The MAM is supplied through the MAM feeder 110. A vacuum is applied to the synthesis reactor 100 to fill the synthesis reactor 100 with methanol and a catalyst. The temperature of the synthetic reactor 100 is adjusted to 40 ° C. by using a hot water tank or the like, and the MAM is dropped through the MAM feeder 110. The drop-in time is about 10 minutes. When the reaction starts, heat is generated and the temperature rises. It is safe to control the reaction to proceed at a temperature of about 40 to 60 占 폚. Since the reaction is equilibrated in approximately 20 to 45 minutes, a portion of the material in the synthesis reactor 100 is sampled through the reaction sampler 140 at the time of the approximate equilibrium, and GC analysis and moisture analysis are performed. As a result of analysis, when the conversion rate of MMP is 98% or less, water is supplied through the water supplier 150 and the reaction is further performed for about 20 minutes. The supply of moisture is controlled in the range of 100 ppm to 200 ppm. After the reaction for 20 minutes, the conversion rate and moisture content are analyzed again through the reaction sampler 140. If the conversion rate of MMP is 98% or less, the above water addition reaction process is repeated. If necessary, the reaction process can be recirculated through control of various valves. If a sufficient conversion rate is achieved, the reactants are transferred through the synthesis reactant outlet 160 for the next process.

FIG. 2 is a schematic view showing a reaction process of the neutralization control unit as part of an apparatus for producing methyl methoxypropionate according to the present invention. FIG. The reactants transferred from the synthesis control unit are supplied to the neutralization reactor 200 through the synthesis reactant inlet 210. The basic catalyst is neutralized by supplying sulfuric acid through the neutralizer feeder 220. The neutralization reaction may be carried out for about 30 minutes. Acidity can be measured to see if sufficient neutralization has occurred and, if necessary, additional neutralizing agent supply and reaction can be performed. The neutralization reaction is complete and the neutralization reactions are transferred through the neutralization reactant outlet 230 for the next process (distillation).

3 is a schematic diagram showing a first distillation apparatus section as a part of an apparatus for producing methyl methoxypropionate according to the present invention. MMP, MAM, sulfuric acid and the like are present together with methanol in the neutralization reactant. The boiling point of methanol is about 64.7 ° C, the boiling point of MAM is 80.5 ° C, the boiling point of MMP is about 143 ° C, and the boiling point of sulfuric acid is about 317 ° C. The primary goal of the first distillation unit is to separate materials with relatively low boiling points, the main target being methanol. The first distillation unit includes a first evaporator 330, a first distillation column 320, a first condenser 340, a second condenser 350, and a first condenser 360. The neutralization reaction product is received from the neutralization control unit and is first stored in the first service tank 310 through the neutralization reaction product inlet 300. The neutralization reactant is sent from the first service tank 310 to the first evaporator 330 and the first evaporator 330 is heated to evaporate the substances in the first distillation column 320. Once the temperature has risen to some extent, it is possible to circulate the neutralization reactants from the first service tank 310 to the first distillation column 320 for the sake of efficiency so that they are returned to the first evaporator 330. By adjusting the temperature to a predetermined temperature, substances having a relatively low boiling point are collected in the first distillation column 320 and materials having a relatively high boiling point are collected in the first evaporator 330. Methanol is sent to the first condenser 340 in a gaseous state through the first distillation column 320 composed of a plurality of stages and is condensed. In this process, the purity is checked. If the purity is below a certain level, And the distillation process can be repeated. If the purity is above a certain level, it is sent from the first condenser 340 back to the second condenser 350. The purity is checked, and if it is satisfactory, the methanol is stabilized through the first cooler 360, stored in the first storage tank 370, and reusable with methanol. The purity is checked to be not satisfactory, and the distillation process can be repeated by sending it to the first distillation column 320 again. Meanwhile, the temperature of the first evaporator 330 may be increased to remove relatively low boiling point materials such as excess MAM. Although not shown in the figure, it can be removed through a scrubber or the like which removes impurities. Of course, in the second distillation process, it is more preferable to remove the substances having boiling point higher than methanol but lower than MMP through the scrubber in the process of raising the temperature. This is because, in the first distillation process, it is aimed to recover methanol by focusing on it, so that the possibility of containing impurities in the process of raising the temperature more than necessary is increased, and the possibility of repeating unnecessary processes for securing purity is increased to be. When the methanol recovery process is completed, high boiling point materials remain in the first evaporator 330 and they are transferred to the second storage tank 380 for a secondary distillation process.

FIG. 4 is a schematic view showing a second distillation unit as a part of an apparatus for producing methyl methoxypropionate according to the present invention, in a form similar to that of the first distillation unit. The second distillation unit includes a second evaporator 430, a second distillation column 420, a third condenser 440, a fourth condenser 450, a second condenser 460, and a second condenser 460 for the purpose of recovering the MMP. And a third cooler 480. Distilled materials from the first distillation unit are stored in the second service tank 410 through the second storage tank outlet 400. In the second service tank 410, the stored substance is sent to the second evaporator 430 and the second evaporator 430 is heated to evaporate the substances in the second distillation column 420. Similar to the first distillation process, when the temperature is raised to some extent, it may be circulated from the second service tank 410 directly to the second distillation column 420 for efficiency. The MMP can be collected in the second distillation column 420 and the MMP can be separated into the third condenser 440 and the fourth condenser 450 through the second distillation column 420, And then sent to the second cooler 460 to be stabilized by the MMP to store the MMP in the third storage tank 470. Likewise, the purity is checked in the condensation process and sent to the second distillation column 420 to repeat the distillation process to increase the purity. Meanwhile, in the process of heating the second evaporator 430 to raise the temperature, the MAM having a lower boiling point than the MMP can be removed through the scrubber. Materials having a relatively higher boiling point than the MMP remain in the second evaporator 430. They are stabilized through the third cooler 480 and moved to the impurity tank 490 to remove it.

In the reaction process and the neutralization process, it is possible to construct the equipment in such a way that the material movement and the circulation process of the process are forced to some extent by using a vacuum pump or the like. In the case of circulation to an evaporator, a distillation column, a condenser, It is possible to apply a reflux system in which the natural pressure is applied through the adjustment of the valve. Meanwhile, in each process, through the process of removing impurities through a scrubber, the equipment of the present invention and the reaction process through a multi-stage distillation process and a repeating cycle process, impurities such as VOCs And the content can be reliably reduced.

The following examples illustrate the invention. The following examples should not be construed as limiting the scope of the present invention and should be construed to facilitate understanding of the present invention. The test scale was pilot scale.

<Examples>

28.2 L of methanol was charged to the reactor and 31.4 L of MAM was charged to the feeder. About 696 moles and about 348 moles, respectively, at a molar ratio of about 2: 1. 100 g of sodium methoxide was dissolved in methanol and placed in the reactor. The temperature of the reactor was adjusted to 40 캜 by using a hot water tank. The MAM was added dropwise over 10 minutes using the feeder valve. After the start of the reaction, the sample was first sampled in about 30 minutes, and analyzed by GC and moisture. The conversion rate was about 87%, and the water content was 48 ppm. Thus, the water was added at 135 ppm and further reacted for 20 minutes. The reaction temperature was adjusted within the range of 54 to 60 占 폚.

After the additional reaction, the second sample was sampled and the conversion rate was 95.40%. The water was added again at 125 ppm and further reacted for 20 minutes. The conversion rate was 98.6%. The reaction process was then stopped, cooled to 35 &lt; 0 &gt; C and transferred to another reactor. The catalyst was neutralized using 78 mL of 50% H ₂ SO ₄ in MeOH. The neutralization reaction proceeded for about 30 minutes. The acidity was measured by sampling and it was confirmed that neutralization was properly performed. The reactants were subjected to fractional distillation for primary methanol separation and fractional distillation for secondary MMP separation. ICP analysis was performed on isolated MMPs. The content of sodium was less than 1 ppb, satisfying the reference value of 20 ppb or less, and the other impurity metal contents were all less than 1 ppb, resulting in a high purity product with almost no impurities.

<Comparative Example>

28.2 L of methanol was charged to the reactor and 31.4 L of MAM was charged to the feeder. About 696 moles and about 348 moles, respectively, at a molar ratio of about 2: 1. 100 g of sodium methoxide was dissolved in methanol and placed in the reactor. The temperature of the reactor was adjusted to 40 캜 by using a hot water tank. The MAM was added dropwise over 10 minutes using the feeder valve. The reaction time was about 70 minutes. The conversion rate was measured by sampling, and the conversion rate was about 90%. The reaction process was then stopped, cooled to 35 &lt; 0 &gt; C and transferred to another reactor. The catalyst was neutralized using 78 mL of 50% H ₂ SO ₄ in MeOH. The neutralization reaction proceeded for about 30 minutes. The acidity was measured by sampling and it was confirmed that neutralization was properly performed. The reactants were subjected to fractional distillation for primary methanol separation and fractional distillation for secondary MMP separation.

The production method in the case where the water addition process of the present invention is carried out and the equipment for carrying out this process are inventions which can obtain high purity and high yield.

While the present invention has been particularly shown and described with reference to exemplary embodiments, it is to be understood that the invention is not limited to the disclosed exemplary embodiments, but, on the contrary, is intended to cover various modifications and equivalent arrangements included within the spirit and scope of the appended claims. You must understand that you can do it.

100: Synthesis reactor 110: MAM feeder
120: methanol feeder 130: catalyst feeder
140: Reaction sampler 150: Moisture feeder
160: Synthetic Reactor Outlet
200: neutralization reactor 210: synthesis reactant inlet
220: neutralizer feeder 230: neutralization reactant outlet
300: neutralization reactant inlet 310: first service tank
320: first distillation column 330: first evaporator
340: first condenser 350: second condenser
360: first cooler 370: first storage tank
380: Second storage tank
400: second storage tank outlet 410: second service tank
420: second distillation column 430: second evaporator
440: Third condenser 450: Fourth condenser
460: second cooler 470: third storage tank
480: third cooler 490: impurity tank

Claims (10)

A method for producing methyl methoxypropionate (MMP) by reacting methyl acrylate with methanol using an alkali metal alkoxide as a catalyst,
Further comprising the step of supplying water to the reaction to increase the conversion of the MMP,
The process comprises sampling the reactant between 20 minutes and 45 minutes after the start of the reaction between the metal acrylate and the methanol to measure the moisture content of the reactant, and when the moisture content is less than 100 ppm, the range is from 100 ppm to 200 ppm Is based on the weight of water in the reactant). &Lt; RTI ID = 0.0 &gt; 11. &lt; / RTI &gt;
delete delete delete The method according to claim 1,
Wherein the alkali metal alkoxide catalyst is sodium methoxide. I) reacting methylacrylate with methanol using sodium methoxide as a catalyst;
Ii) measuring the moisture content of the reactant by sampling the reactant between 20 minutes and 45 minutes after initiation of the reaction of step i);
Iii) supplying water so that the water content in the step ii) is less than 100 ppm, the water content is in the range of 100 ppm to 200 ppm (ppm is based on the weight of water in the reactant);
Iv) neutralizing the catalyst by adding an acid to the reactant; And
And (v) distilling the reaction product. The method for producing methylmethoxypropionate (MMP) An apparatus for producing methyl methoxypropionate (MMP) by reacting methyl acrylate with methanol using an alkali metal alkoxide as a catalyst,
A synthesis control unit for reacting methyl acrylate with methanol using an alkali metal alkoxide as a catalyst;
A neutralization regulator unit in which substances in the synthesis regulator unit are moved to neutralize the catalyst;
A first distillation unit for separating substances having a low boiling point by moving the substances of the neutralization control unit; And
And a second distillation unit in which materials remaining in the first distillation unit are moved to perform separation of the MMP,
Wherein the synthesis control unit comprises a reaction sampler for confirming the water content in the reaction product of methyl acrylate and methanol and a water supply unit for supplying water to the reaction product of the synthesis control unit.
delete delete delete

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